Korean Journal of Food Science and Technology (한국식품과학회지)

Korean Society of Food Science and Technology (한국식품과학회)
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Development and Validation of an Analytical Method for the Insecticide Sulfoxaflor in Agricultural Commodities using HPLC-UVD

HPLC-UVD를 이용한 농산물 중 살충제 sulfoxaflor의 시험법 개발 및 검증

  • Do, Jung-Ah (Food Chemical Residues Division, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Food and Drug Administration) ;
  • Lee, Mi-Young (Food Chemical Residues Division, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Food and Drug Administration) ;
  • Park, Hyejin (Food Chemical Residues Division, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Food and Drug Administration) ;
  • Kwon, Ji-Eun (Food Chemical Residues Division, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Food and Drug Administration) ;
  • Jang, Hyojin (Food Chemical Residues Division, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Food and Drug Administration) ;
  • Cho, Yoon-Jae (Food Chemical Residues Division, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Food and Drug Administration) ;
  • Kang, Il-Hyun (Food Chemical Residues Division, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Food and Drug Administration) ;
  • Lee, Sang-Mok (Food Chemical Residues Division, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Food and Drug Administration) ;
  • Chang, Moon-Ik (Food Chemical Residues Division, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Food and Drug Administration) ;
  • Oh, Jae-Ho (Food Chemical Residues Division, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Food and Drug Administration) ;
  • Hwang, In-Gyun (Food Chemical Residues Division, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Food and Drug Administration)
  • 도정아 (식품의약품안전청 식품의약품안전평가원 식품위해평가부 화학물질과) ;
  • 이미영 (식품의약품안전청 식품의약품안전평가원 식품위해평가부 화학물질과) ;
  • 박혜진 (식품의약품안전청 식품의약품안전평가원 식품위해평가부 화학물질과) ;
  • 권지은 (식품의약품안전청 식품의약품안전평가원 식품위해평가부 화학물질과) ;
  • 장효진 (식품의약품안전청 식품의약품안전평가원 식품위해평가부 화학물질과) ;
  • 조윤제 (식품의약품안전청 식품의약품안전평가원 식품위해평가부 화학물질과) ;
  • 강일현 (식품의약품안전청 식품의약품안전평가원 식품위해평가부 화학물질과) ;
  • 이상목 (식품의약품안전청 식품의약품안전평가원 식품위해평가부 화학물질과) ;
  • 장문익 (식품의약품안전청 식품의약품안전평가원 식품위해평가부 화학물질과) ;
  • 오재호 (식품의약품안전청 식품의약품안전평가원 식품위해평가부 화학물질과) ;
  • 황인균 (식품의약품안전청 식품의약품안전평가원 식품위해평가부 화학물질과)
  • Received : 2012.09.28
  • Accepted : 2013.01.05
  • Published : 2013.04.30
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Abstract

Sulfoxaflor is a new active ingredient within the sulfoximine insecticide class that acts via a unique interaction with the nicotinic receptor. The MRLs (maximun residue limit) of sulfoxaflor in apple and pear are set at 0.4 mg/kg and that in pepper is set at 0.5 mg/kg. The purpose of this study was to develop an analytical method for the determination of sulfoxaflor residues in agricultural commodities using HPLC-UVD and LC-MS. The analysis of sulfoxaflor was performed by reverse phase-HPLC using an UV detector. Acetone and methanol were used for the extraction and aminopropyl ($NH_2$) cartridge was used for the clean-up in the samples. Recovery experiments were conducted on 7 representative agricultural products to validate the analytical method. The recoveries of the proposed method ranged from 82.8% to 108.2% and relative standard deviations were less than 10%. Finally, LC-MS with selected ion monitoring was also applied to confirm the suspected residues of sulfoxaflor in agricultural commodities.

국내 신규 살충제로 등록되어진 sulfoxaflor에 대해 농산물 중 잔류실태를 조사하기 위하여 HPLC-UVD와 LC-MS를 이용한 시험법을 개발하였다. Sulfoxaflor 시험법의 회수율은 시료별 적당한 추출 및 정제 방법을 적용한 결과 현미, 감자, 감귤, 사과, 배, 고추, 대두에서 0.05, 0.4 및 0.5 mg/kg 수준에서 82.8-108.2%이었다. 회수율에 대한 모든 분석오차는 10% 미만으로 CODEX 잔류물질 분석 가이드라인에 만족하였다. 분석을 위한 기기 조건에서 sulfoxaflor의 정량한계는 0.05 mg/kg이었으며 0.1-5.0 mg/kg 범위에서 상관계수($R^2$) 0.999 이상의 높은 직선성을 보여주었다. 따라서 본 연구에서 개발된 잔류농약 시험법은 농산물을 대상으로 효과적인 시료 전처리 방법과 최적의 정제 과정을 확립하여 다양한 농산물에 대한 잔류량 검출이 적당함을 확인할 수 있었다. 이와 같이 확립한 sulfoxaflor의 잔류시험법은 국제적 분석 기준을 만족할 뿐만 아니라 LC-MS를 이용한 잔류분의 재확인한 결과를 살펴볼 때 분석과정의 신뢰성 또한 확보할 수 있어 식품공전 공정시험법으로 사용될 것이다.

Keywords

References

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